CN1355776A - Low expansion, high porosity, high strength cordierte body and making method thereof - Google Patents

Low expansion, high porosity, high strength cordierte body and making method thereof Download PDF

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CN1355776A
CN1355776A CN00808790A CN00808790A CN1355776A CN 1355776 A CN1355776 A CN 1355776A CN 00808790 A CN00808790 A CN 00808790A CN 00808790 A CN00808790 A CN 00808790A CN 1355776 A CN1355776 A CN 1355776A
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ceramic article
microns
cordierite
hole
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CN1166584C (en
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D·M·比尔
C·J·玛拉凯
G·A·默克尔
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Corning Inc
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0006—Honeycomb structures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00129—Extrudable mixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/0037—Materials containing oriented fillers or elements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0081—Uses not provided for elsewhere in C04B2111/00 as catalysts or catalyst carriers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/32—Expansion-inhibited materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24149—Honeycomb-like
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24273—Structurally defined web or sheet [e.g., overall dimension, etc.] including aperture

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  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)
  • Exhaust Gas After Treatment (AREA)
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  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

A sintered ceramic that exhibits an average linear coefficient of thermal expansion (25-800 DEG C) below about 5.0x10<-7>/DEG C, a total porosity between the range of 20% to about 30%. Furthermore, the sintered ceramic article exhibits a pore size distribution such that at least about 86% of pores are of a pore size of less than about 2 mu m. Lastly, the ceramic article exhibits an interconnected pore structure with the pores exhibiting a generally elongated shape, i.e., the pores are predominately oriented with their long axis in the plane of the webs. This invention also relates to a method for producing a sintered cordierite ceramic article involving first compounding and plasticizing a cordierite-forming inorganic powder batch comprising a platy talc having median particle of size less than about 2 mu m, and preferably a talc morphology index greater than about 0.75. The batch further comprises at least 4% by weight of the inorganic powder batch mixture of a dispersible A12O3-forming source having a specific surface area in excess of 50m<2>/g and one or more of the components of kaolin, calcined kaolin, silica dioxide, and corundum, each having a median particle sizes less than 5 mu m. The plasticized powder batch thus provided is next formed into a green honeycomb by extrusion through a honeycomb extrusion die and the green honeycomb is fired to a temperature and for a time sufficient to convert the green honeycomb into a crystallized cordierite ceramic article having the aforementioned properties.

Description

Low expansion, high porosity, high strength cordierte body and manufacture method thereof
The present invention requires people such as Beall to be entitled as " low expansion, high porosity, high strength cordierte body and manufacture method thereof ", respectively at the U.S. Provisional Application No.60/138 that submits on June 11st, 1999 and on December 30th, 1999,930 and No.60/174,010 right of priority.
Background of invention
1. invention field
The present invention relates to cordierite ceramic body as support of the catalyst, be specifically related to such cordierite bodies, it has the superperformance of high thermal-shock resistance and good available high surface area activated alumina slurries coating, the former is based on its low thermal coefficient of expansion (CTE), and the latter is based on its high pore rate and the very thin narrow pore size distribution that is generally slot.
2. prior art
The waste gas that the combustion system of use hydrocarbon fuel such as appropriate hydrocarbon gas, gasoline or diesel oil is emitted can cause serious pollution to atmosphere.In the middle of many pollutents in these waste gas hydrocarbon and oxygenatedchemicals are arranged, the latter comprises nitrogen oxide (NOx) and carbon monoxide (CO).Automotive industry manages to reduce the amount of the pollutent of being discharged by automobile engine system for many years, and first automobile that is equipped with catalytic converter is introduced to the market at twentieth century the mid-1970s.
General type is the base material that the cordierite substrates of honeycomb is preferably used as the catalytic active component that catalytic converter is used on the bearing automobile very early, and some reasons are that the thermal-shock resistance of cordierite ceramic is very high.Ceramic honey comb with low thermal coefficient of expansion, high porosity and high strength over-all properties is especially noticeable as the base material of the high-performing car catalytic converter with thin-walled honeycomb.The demand that the thin trichroite monolithic of netting is arranged is increased, require the transformation efficiency of the catalytic converter on the automobile market higher relevant with legislation.Thin net can reduce the base material quality, starts faster.In addition, the base material quality need be do not increased, just geometrical surface can be increased.Another advantage of thin-walled substrates is that back pressure is less.
Though the thin wall cordierite honeycomb has these advantages, the wall thickness of honeycomb reduces, and can reduce honeycomb strength.This has just caused the problem of installation aspect.If intensity reduces a lot, will cause base material in the installation process and break.Therefore, when wall thickness is very thin, just require strength of materials height, reduce to offset the geometry intensity that is run into.But in order to have the screening characteristics of high high surface area alumina washcoat coating, high porosity is arranged preferably, described washcoat coating is applied on the incinerating base material.In addition, high porosity can reduce the thermal mass of base material, and makes time of startup katalysis of catalytic converter faster.Low thermal coefficient of expansion is to preventing that base material is owing to thermal shocking is ruptured very important.Unfortunately, known high porosity and low thermal coefficient of expansion can reduce the intensity of cordierite honeycomb.Exist in the tiny crack that forms owing to anisotropic thermal expansion in the process of cooling in the general cordierite substrates, will have low heat expansion property.The tiny crack that exists in the cordierite substrates is used to limit the intensity of cordierite bodies.High porosity in the base material is limiting material intensity also, because hole descends the section area that bears load.
United States Patent (USP) № 4849275 (authorizing people such as Hamaguchi) has disclosed a kind of cordierite honeycomb structure body, its porosity is 30-42%, and the intravital aperture of structure is that the percentage that the hole of 0.5-5.0 micron accounts for all hole cumulative volumes is not less than 70%, preferably is not less than 80%.United States Patent (USP) № 4869944 (authorizing people such as Harada) has disclosed a kind of cordierite bodies, and its axial CTE is not more than 3 * 10 -7/ ℃, porosity is 30-42%, and hole wherein 〉=40% is the 0.5-5.0 micron, and≤30% hole is 〉=10 microns.Narrow pore distributes and enough low CTE though these documents have all disclosed, but overall porosity surpasses 30%, and their not announcements, also shows without any embodiment, the narrow pore size distribution in enough thin elongated orientation hole, such hole are that preparation has less than 5 * 10 -7/ ℃ low CTE and the sufficiently high cordierite bodies of intensity necessary.
United States Patent (USP) № 4877670 (authorizing Hamanaka) has disclosed a kind of cordierite bodies, and it has less than 10 * 10 -7/ ℃ low CTE and greater than 5 microns, be preferably greater than 2 microns low hole cumulative volume.Though the document has disclosed the close limit pore, it does not have to disclose the combination with narrow distribution fine pore, discloses yet and requires elongated orientation hole, and such hole has high strength and less than 5 * 10 to guaranteeing to form -7/ ℃ the cordierite bodies of over-all properties of low CTE be essential.
U.S. Patent application № 09/348307 (people such as Merkel) has disclosed such cordierite bodies, its CTE≤4 * 10 -7/ ℃, the median size at least 85% hole is the 0.5-5.0 micron.This patent has also disclosed second embodiment, comprises a kind of cordierite bodies, and its CTE is 4-6 * 10 -7/ ℃, overall porosity is at least 30 volume %, and the aperture at least 85% hole is the 0.5-5.0 micron.The document has disclosed narrow distribution pore once more, but does not disclose elongated orientation pore structure and narrow distribution fine pore, and it is necessary that this is that preparation has a trichroite of high strength and low CTE over-all properties.
Therefore, the purpose of this invention is to provide improved cordierite ceramic and preparation method thereof, this cordierite ceramic demonstrates the narrow pore size distribution of low-thermal-expansion, high porosity, high strength and elongated orientation aperture.
The general introduction of invention
The invention provides a kind of agglomerating ceramic base material and preparation method thereof, this base material has the primary crystallization phase that contains trichroite, and its thermal expansion is low and the overall porosity height.Described hole contains such fine porosity uniquely, and it has narrow pore size distribution, and is generally elongated shape, it is believed that it is of value to the unexpected high intensity of these low CTE base materials.
Specifically, the average thermal linear expansion coefficient of 25 °-800 ℃ of agglomerating ceramics of the present invention is less than about 5.0 * 10 -7/ ℃, overall porosity is 20-about 30%.In addition, the pore size distribution of this sintered ceramic product is, at least about the aperture in 86% hole less than about 2 microns.Final ceramic demonstrates the pore texture that interpenetrates, and hole is roughly elongated shape, and hole is orientated mostly, and the hole major axis is in the plane of net.
The present invention also relates to the preparation method of agglomerating cordierite ceramic article, comprise the inorganic powder batch of at first mixing and plastifying the formation trichroite, it contains median particle diameter less than about 2 microns talcum, and morphological indices is preferably greater than about 0.75 foliated talc.This batch of material also contains the specific surface area that accounts for inorganic powder mixture 4% (weight) at least and surpasses 50m 2The formation of/g can disperse Al 2O 3The source material and one or more compositions in kaolin, incinerating kaolin, silicon-dioxide and the corundum, every person's median particle diameter is all less than 5 microns.
Then, from cellular extruding die orifice, extrude the plasticizing Powder batch material that obtains like this, form green honeycomb, in certain temperature calcining for some time, the crystallization cordierite ceramic article that this time should be enough to that green honeycomb is changed into and has aforementioned properties.
Brief description of drawings
Fig. 1 is that cordierite bodies of the present invention amplifies 500 times electron scanning micrograph;
Fig. 2 is that the comparative cordierite body of composition 2 amplifies 500 times electron scanning micrograph;
Fig. 3 is that the accumulation pressure-bearing of the embodiment of the invention 1 and two Comparative Examples 2 and 3 is gone into the graph of a relation between volume and the aperture.
Detailed description of the invention
Cordierite bodies of the present invention has made up the following compelling performance of thin wall cordierite honeycomb ceramics: applying property, the pore structure that interpenetrates and the high strength of good thermal-shock resistance, good aluminium oxide washcoat coating, the first performance is based on its low thermal coefficient of expansion (CTE), less than about 5.0 * 10-7/ ℃, the second performance is based on its high overall porosity (＞20%, but less than 30%), the 4th kind of performance is based on the pore-size distribution of its pinhole, this distributes specifically, and less than about 2 microns, there is the degree of orientation in the hole simultaneously at least about the average pore size in 86% hole, the main spread pattern in hole is that major axis is positioned at the plane of net. According to the present invention, CTE is the average swell value that is recorded between 25-800 ℃ by dilatometry, about honeycomb, is the average swell value that is parallel to the length direction that opens wide conduit.
The shape in hole and orientation are influential to the intensity of cordierite honeycomb. Contain orientation and be improved perpendicular to the cordierite bodies that the strength ratio of the cordierite bodies of the elongated hole that applies power contains randomly-oriented spherical pore, reduced because stress is concentrated.
In order to obtain to have the cordierite bodies of above-mentioned unique combination property, the interior essential employing average grain diameter of mixture in batches is very thin, the particular composition of high surface raw material. Particle diameter used herein is represented by average grain diameter, is recorded by the centrifugation technology.
According to the present invention, a kind of plasticization mixture for the preparation of above-mentioned ceramic is provided, this mixture contains: (a) median particle diameter is less than about 2 microns very thin talcum powder, and (b) formation can disperse Al2O 3The source material, be selected from the hydroxide of transition alumina, aluminium hydroxide or aluminium oxide, this Al2O 3The specific area of source material surpasses 50m2/ g accounts for 4% (weight) of plasticization inorganic mixture at least, and (c) one or more compositions in the kaolin of kaolin, calcining, silica and the corundum, every person's median particle diameter are all preferably less than 5 microns.
In a preferred implementation, talcum is a sheet, and promptly the talcum form is a platelet particles, that is to say, its particle is two-dimension sizes to be grown and the short particle of one dimension size, in other words, is long and wide all much bigger than thickness small thin slices.This talcum preferably has the morphological indices greater than about 0.75.Morphological indices (seeing United States Patent (USP) 5,141,686) is a kind of measurement of talcum flatness.Measuring an exemplary process of morphological indices, is that sample is inserted in the specimen holder, makes the degree of orientation of foliated talc reach maximum on the in-plane of specimen holder.Talcum to this orientation carries out X-ray diffraction mensuration then.Morphological indices by the following formula sxemiquantitative set up the relation of this steatitic flat features and XRD peak intensity: M = I x I x + 2 I y In the formula, I xThe peak that is (004) is strong, I yThe peak that is (020) reflection is strong.
Form Al 2O 3The source material be meant Al 2O 3Can change into Al when self or calcining 2O 3The low other materials of water solubility.Some form Al 2O 3The exemplary source material comprise aluminum oxide, Al (OH) 3The oxyhydroxide of (being also referred to as aluminum trihydrate or gibbsite thing) or aluminum oxide (being also referred to as single hydrated aluminum or boehmite mineral or pseudobochmite).
Form high surface area and can disperse Al 2O 3Component or source material can provide with powdery or solation.Can disperse to be meant that very the granule of fine particles can be broken, and can be scattered in median particle diameter less than in other about 0.3 micron component particles.High surface area refers to that surface-area is greater than 50m 2/ g is more preferably greater than about 100m 2/ g.Such powder can comprise boehmite, pseudobochmite, γ-phase alumina, δ-phase alumina or be called the unclassified stores of transitional alumina.One preferred embodiment in, form high surface area and can disperse Al 2O 3Composition or source material contain surface-area and surpass 150m 2The boehmite of/g.
In order to realize purpose of the present invention, formation can disperse Al 2O 3The source material be that heating the time can form Al 2O 3Compound.
If kaolin exists, its median particle diameter should be about the 0.2-2.0 micron, should account for below about 35% (weight) of a collection of raw material total amount.Be used for forming the Al of trichroite 2O 3Surplus by through incinerating kaolin or form Al 2O 3The source material SiO is provided 2Surplus by providing through incinerating kaolin or silicon dioxide powder.The existence form of silicon-dioxide the silicon dioxide granule (＞50m that preferably surface-area is very high 2/ gm).If use through calcined clay, it should be very thin, and preferred median size is more preferably less than 1 micron less than 2 microns, and surface-area is greater than 10m 2/ gm.
Above-mentioned raw materials that the plasticization mixture is used uniform mixing in addition in a mixing step makes to react completely in their heat treatment processes afterwards.Add a kind of tackiness agent system this moment, so as to form can be shaped, can molded, squeezable mixture.The used a kind of preferable tackiness agent system of the present invention comprises the cellulose ether binder component that is selected from methylcellulose gum, methylcellulose gum derivative and their mixture, and surface active agent composition is preferably stearic acid or sodium stearate, and aqueous solvent.Use a kind of like this tackiness agent system to obtain good effect, by raw mixs such as 100 weight part inorganicss, the source material that forms aluminum oxide and silicon-dioxide and talcums, its content is: about 0.2-2 weight part sodium stearate, about 2.5-6.0 weight part methylcellulose gum or Vltra tears tackiness agent, about 20-50 weight parts water.
In another embodiment, a kind ofly be used for preferred adhesive system of the present invention and comprise the cellulose ether binder component that is selected from methylcellulose gum, methylcellulose gum derivative and their mixture, the non-solvent component that contains poly-alpha olefins, be selected from the surface active agent composition of stearic acid, Texapon Special, lauric acid, oleic acid, palmitinic acid and composition thereof, and aqueous solvent.Use a kind of like this tackiness agent system to obtain good effect, by 100 weight part inorganic raw material mixtures, its content is as described below: about 2-10 weight part poly-alpha olefins, about 0.2-2 weight part surface active agent composition, about 2.5-5.0 weight part Vltra tears tackiness agent, about 8-25 weight parts water.
Each component of tackiness agent system is mixed with known appropriate method with a certain amount of inorganic powder, and with for example method of extruding, preparation can form the stupalith of ceramic body and the intimate mixture of tackiness agent system.With any known method that forms pottery, methods such as for example extruding, injection-molded, streamer, centrifugal casting, pressure injection, dry-pressing are configured as green compact to the tight and uniform squeezable compound of gained then.Be suitable for the thin-walled honeycomb base material of making support of the catalyst, the preferably method of extruding from die orifice for preparation.The ceramic green of making dry then and under high enough temp the sufficiently long time of calcining, obtaining trichroite is the burning ceramics body of primary crystallization phase.Dry and calcination condition can become with processing conditions, as concrete composition, green compact size and equipment characteristic.
Dry available any ordinary method is carried out, for example hot-air dry or radio-frequency drying.Preferable methods is a radio-frequency drying.
The calcination temperature range that forms cordierite bodies should be 1340 °-1440 ℃, wants sufficiently long in soaking time, makes the reaction that forms the trichroite phase carry out fully substantially.The calcined body that forms preferably contains at least about 95% (weight) trichroite.
In order to further specify principle of the present invention, the present invention also comprises embodiment and two Comparative Examples of cordierite bodies of the present invention.But, understand that this embodiment only is used for explanation, does not limit the present invention.Do not breaking away under the spirit and scope of the present invention situation, can carry out various variations and change the present invention.
Embodiment
Be suitable for generating the inorganic powder compound of trichroite as the ceramic body of its primary crystallization phase, its composition is listed in the table 1 with weight percentage, and is as shown in table 1.By mixing and doing the component of mixing the appointment inorganic mixture shown in the Table I, prepare a collection of mixture of the present composition 1 and Comparative composition 2.Be noted that it is 180m that composition 1 contains surface-area 2The boehmite of/g and morphological indices are 0.91 foliated talc, and Comparative composition 2 does not have polymolecularity Al 2O 3, and talcum morphological indices wherein is the talcum of 0.7-0.75.Add consumption organic binder bond system as shown in Table I in these mixtures, afterwards, these intermediate mixture are further mixed with deionized water, form the plastifying ceramic mixture.The parts by weight that the component of tackiness agent system as shown in Table I is is benchmark with 100 parts of inorganics total amounts.Table I has also shown the median size (micron) of the raw material of the purchase that is used for material.All particle diameters that are noted that composition 1 all are the median sizes of submicron, and it is 6 microns talcum that 2 of Comparative composition contain median size.
Through the plastifying compound,, have 816 honeycomb/inches of about 3.0 inch diameters and 2.72 mil thickness of honeycomb walls being suitable for forming about 5 inches long 2The condition of monolith substrate under, extrude from extrusion machine.The green honeycomb that is formed by said composition is removed all water or the liquid phase that may exist through thorough drying, carries out heating and calcining then, and its condition should be enough to remove the organic binder bond system and implement sintering from extruding in rod and the honeycomb.Specifically, green compact all are heated to about 1380 °-1420 ℃, are incubated about 8 hours, and promptly used calcination condition is suitable for forming the ceramic body that trichroite is the primary crystallization phase.
Table I
Form with the batch of material that weight percent is represented
(median particle diameter that records for centrifugal settling method in the bracket, micron)
Raw material Composition 1 of the present invention Comparative composition 2
Inorganics
Talcum 39.95(1.5) 40.86(6.6)
Kaolin 16.55(0.8) 12.04(0.8)
Through incinerating kaolin 24.73(0.8) 29.68(0.8)
Al 2O 3 5.73(0.6) 15.43(0.4)
AlOOH-xH 2O(180m 2/g) 11.05(0.1) --
Silicon-dioxide 2.0(3.8) 2.0(3.8)
Organism
Methylcellulose gum 5.0 3.5
Lubricant 1.0 0.5
Oil 8.0 6.0
Table II has been listed some the selection performances of pottery with the preparing the batch of composition 1 shown in the Table I and Comparative composition 2.3 of Comparative Examples have been listed the representative performance of a series of comparative cordierite bodies, its hole performance is specified in the above-mentioned Hamaguchi document, specifically be that porosity is 30-42%, all hole cumulative volumes are not less than 70%, specifically are that the diameter of 71-73% is the hole of 0.5-5.0 micron in the cordierite bodies.The performance that each ceramic body is listed in be rod the breaking tenacity modulus (MOR, psi), the mean thermal expansion coefficients (CTE) (* 10 of rod in about 25-800 ℃ temperature range -7℃), the overall porosity (volume %) of pottery and median size be less than 2 microns porosity, these two kinds of hole performances all use pressure Hg method hole tester to record.In addition, Table I has also been listed the ultimate compression strength of hydrostatic pressure intensity and A, B and C axle in, and the unit of measure of these performances all is psi.
Table III
Composition 1 Comparative composition 2 Comparative Examples 3
Performance through the incinerating cordierite bodies
Cellular densities 816 900 811
Honeycomb wall thickness 2.72 2.70 2.72
?CTE 3.7 5.0 3.2
Porosity % 26.8 25.3 31.9
Porosity less than 2 microns 92 41 20-22
MOR(psi) 361 288 270
Hydrostatic pressure intensity FN (psi) 200 145 75
A axle ultimate compression strength (psi) 3640 2120 1190
B axle ultimate compression strength (psi) 313 224 86
C axle ultimate compression strength (psi) 25 31 11
Test result in the table shows, the porosity of right that sample of the present invention has had requirement comprises that overall porosity is that 20%-is about 30%, and is concrete 26.8%, pore size distribution be make at least about 86%, the aperture in concrete 92% hole is less than about 2 microns.In addition, sample of the present invention shows low CTE, is 3.7 * 10/ ℃, demonstrates sufficiently high intensity simultaneously, is 361psi.On the other hand, the comparative sample aperture far below sample of the present invention, is respectively 41% and 19% less than 2 micron pore size percentage, and simultaneously intensity is lower, is 270 and 288psi.
Fig. 1 amplifies 500 times SEM with the ceramic body polishing section that above-mentioned composition 1 is made, and it is a 900cpsi cordierite honeycomb structure body, net wall thickness 0.0027inch.Fig. 1 demonstrates a kind of pore structure, and it is the longilineal structure along the hole that the ceramic body net plane is orientated of being roughly of narrow distribution.Fig. 1 has specifically shown the median size that is recorded by Hg platen press hole tester just less than 1 micron, seldom finds to have macropore in this structure.
Fig. 2 is that the ceramic body polishing section of Comparative Examples 3 amplifies 500 times SEM, has formed a 900cpsi cordierite honeycomb structure body once more, and thickness of honeycomb wall 0.0027inch is to obtain the porosity that above-mentioned Hamaguchi document is described in detail.Fig. 2 demonstrates a kind of structure in spheric hole that probably is, not special elongation in hole or orientation.Fig. 2 has specifically shown by Hg porosity testing method and has recorded median size greater than 3 microns, as can be seen, is permitted the porous aperture up to 30 microns; The existence in these holes may be relevant with the decline of this structure intensity.
Fig. 3 is the figure that concerns between accumulation volume of voids and aperture (pore size distribution) of the cordierite bodies made of present composition embodiment 1 (being designated as the curve of A) and two comparative cordierite bodies (be designated as the curve of B and C, distribute corresponding to Comparative Examples 2 and 3).Data shown in this figure record with Hg porosity testing method.O'clock invade volume on the curve corresponding to 40,20,10,5,2 and 0.5 microns accumulation.As can be seen, the size distribution of structure of the present invention (curve A) is much narrower than each comparison structure body from the curve.In fact, find nearly all hole all less than 2 microns, the distribution of comparison structure body is wide, and the volume in the hole more than 2 microns is very big.
Should be appreciated that, though the present invention has been made detailed description in conjunction with some illustrative specific embodiments, but the present invention should not be considered to be subjected to the restriction of these embodiments, because under the present invention's spirit that does not depart from appended claims and limited and wide region situation, can carry out many changes.

Claims (15)

  1. One kind through the calcining extrusion molding cordierite ceramic article, its 25 °-800 ℃ average thermal linear expansion coefficient is less than about 5.0 * 10 -7/ ℃, overall porosity is that 20-is about 30%, its pore size distribution is that aperture at least about 86% hole is less than about 2 microns.
  2. 2. as claimed in claim 1 through the incinerating cordierite ceramic article, it demonstrates the pore texture that interpenetrates, and hole is roughly elongated shape, and is orientated mostly, and the hole major axis is in the plane of net.
  3. 3. as claimed in claim 1 through the incinerating cordierite ceramic article, its MOR intensity is greater than about 300psi.
  4. 4. as claimed in claim 1 through the incinerating cordierite ceramic article, its A axle ultimate compression strength is greater than 3640psi.
  5. 5. as claimed in claim 1 through the incinerating cordierite ceramic article, its overall porosity is 23-30%.
  6. 6. as claimed in claim 1 through the incinerating cordierite ceramic article, its pore size distribution is that aperture at least about 90% hole is less than about 2 microns.
  7. 7. the preparation method through the cordierite honeycomb articles of calcining extrusion molding comprises the steps:
    (a) mixing and plasticizing form the inorganic powder batch of trichroite, and it contains median particle diameter less than about 2 microns talcum, and the specific surface area that accounts for inorganic powder batch mixtures 4% (weight) at least surpasses 50m 2The formation of/g can disperse Al 2O 3The source material and one or more be selected from the component of kaolin, incinerating kaolin, silicon-dioxide and corundum, every person's median particle diameter is all less than 5 microns;
    (b) the plastifying Powder batch material is extruded from honeycomb extruding die orifice, formed green honeycomb;
    (c) green honeycomb is heated to certain temperature, calcining for some time, the crystalline cordierite ceramic article that this time is enough to that green honeycomb is changed into and has following performance: 25 °-800 ℃ average thermal linear expansion coefficient is less than about 5.0 * 10 -7/ ℃, overall porosity is that 20-is about 30%, pore size distribution is, at least about the aperture in 86% hole less than about 2 microns.
  8. 7. method as claimed in claim 7, wherein said talcum comprise that morphological indices is greater than about 0.75 foliated talc.
  9. 8. method as claimed in claim 7, wherein said formation can disperse Al 2O 3The specific surface area of source material surpass 100m 2/ g.
  10. 9. method as claimed in claim 7, wherein said formation can disperse Al 2O 3The source material be that median size is greater than about 150m 2The boehmite of/g.
  11. 10. method as claimed in claim 7, wherein said crystallization cordierite ceramic article has the pore texture that interpenetrates, and its mesoporosity is roughly elongated shape, great majority are orientated, their major axis is in net plane, and MOR intensity is greater than about 300psi, and A axle ultimate compression strength is greater than 3640psi.
  12. 11. a squeezable mixture, it is used to prepare the base material that trichroite is a prima facies, and it contains the inorganic raw material mixture, and the chemical constitution of this inorganic raw material mixture is as follows: 11-17% (weight) MgO, 33-41% (weight) Al 2O 3And 46-53% (weight) SiO 2, described inorganic raw material mixture contains median particle diameter less than about 2 microns talcum, accounts for inorganic powder batch mixtures 4% (weight) at least and surpasses 50m by specific surface area 2The formation of/g can disperse Al 2O 3The source material and one or more be selected from the composition of kaolin, incinerating kaolin, silicon-dioxide and corundum, every person's median particle diameter is all less than 5 microns.
  13. 12. extrudable mixture as claimed in claim 11, wherein said talcum are morphological indiceses greater than about 0.75 foliated talc.
  14. 13. method as claimed in claim 11, wherein said formation can disperse Al 2O 3The specific surface area of source material surpass 100m 2/ g.
  15. 14. extrudable mixture as claimed in claim 11, wherein said formation can disperse Al 2O 3The source material be that median size is greater than about 150m 2The boehmite of/g.
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